CN109609084B - Silicone sealant and preparation method thereof - Google Patents

Silicone sealant and preparation method thereof Download PDF

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Publication number
CN109609084B
CN109609084B CN201811600829.XA CN201811600829A CN109609084B CN 109609084 B CN109609084 B CN 109609084B CN 201811600829 A CN201811600829 A CN 201811600829A CN 109609084 B CN109609084 B CN 109609084B
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silicone sealant
portions
parts
calcium carbonate
silane
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CN109609084A (en
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周熠
王兵
郑常华
宋立芝
付子恩
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Guangzhou Baiyun Technology Co ltd
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Guangzhou Baiyun Chemical Industry Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Sealing Material Composition (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a silicone sealant and a preparation method thereof. The silicone sealant is prepared from the following raw materials in parts by weight: a, ω -dihydroxy polydimethylsiloxane: 100 parts of ground calcium carbonate: 20-150 parts of fumed silica: 1-20 parts of a plasticizer: 10-60 parts of a chain extender: 2-20 parts of a cross-linking agent: 5-20 parts of a coupling agent: 1-10 parts of a catalyst: 0.01-1 part; the fumed silica is hydrophobically treated fumed silica with dimethyldichlorosilane. The silicone sealant has the advantages of high elongation, low modulus and good adhesion with a concrete pavement, and can still keep good performance after being used for a long time under natural conditions.

Description

Silicone sealant and preparation method thereof
Technical Field
The invention relates to the field of high polymer sealing materials, in particular to a silicone sealant and a preparation method thereof.
Background
The concrete pavement is a strip structure exposed in nature, expansion and contraction internal stress is easily formed between plates, and the concrete pavement is damaged, so that seams with certain widths are arranged at intervals. In order to prevent water leakage and accumulation of foreign matter at the joint, the joint must be sealed. The concrete pavement joint materials currently used in China mainly focus on polysulfide, chloroprene rubber, polyurethane and silicone materials. The silicone sealant is used as a concrete road joint sealing material and has excellent performances of weather aging resistance, high and low temperature resistance, good elastic recovery rate and the like, so that the silicone sealant has great advantages in practical application. However, the silicone sealant adopted by the general technology has low elongation at break, high modulus and poor lasting bonding force with a concrete pavement, is easy to be debonded from a gap interface after long-term use, and cannot completely meet the technical parameter requirements of concrete road joint. Therefore, it is necessary to develop a silicone sealant for concrete roads with excellent properties.
Disclosure of Invention
Based on the above, the invention provides a silicone sealant. The silicone sealant has high elongation and lower modulus, and can still maintain good interfacial adhesion after long-term use.
The specific technical scheme is as follows:
the silicone sealant is prepared from the following raw materials in parts by weight:
a, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 20 to 150 parts of
Gas phase process silica: 1 to 20 parts of
Plasticizer: 10 to 60 portions of
Chain extender: 2 to 20 portions of
A crosslinking agent: 5 to 20 parts of
Coupling agent: 1 to 10 parts of
Catalyst: 0.01-1 part;
the fumed silica is hydrophobically treated fumed silica with dimethyldichlorosilane.
In some embodiments, the silicone sealant is prepared from the following raw materials in parts by weight:
a, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 120 to 140 portions of
Gas phase process silica: 9 to 13 portions of
Plasticizer: 30 to 60 portions of
Chain extender: 2 to 6 portions of
A crosslinking agent: 10 to 14 parts by weight of
Coupling agent: 1 to 3 portions of
Catalyst: 0.05 to 0.15 portion.
In some of these embodiments, the viscosity of the a, ω -dihydroxypolydimethylsiloxane is 20000 to 100000mpa.s at 25 ℃.
In some of these embodiments, the a, ω -dihydroxypolydimethylsiloxane has a viscosity of from 70000 to 90000mpa.s at 25 ℃.
In some of these embodiments, the ground calcium carbonate has an average particle size of 3.5 to 5 μm and a moisture content of less than 0.1%.
In some of the embodiments, the fumed silica has a specific surface area of 150-200 cm2/g
In some of these embodiments, the plasticizer is dimethicone having a viscosity of 100 to 1000mPa.s at 25 ℃.
In some of these embodiments, the plasticizer is dimethicone having a viscosity of 30 to 400mPa.s at 25 ℃.
In some of these embodiments, the crosslinking agent is at least one of methyltributanoxime silane, vinyltributoxime silane, phenyltributoxime silane, and tetrabutoximosilane.
In some of these embodiments, the chain extender is at least one of dimethyldibutylketoximosilane, methylvinyldibutylketoximosilane, methylvinylbis (methylisobutylketonoximino) silane, and methylvinyldiacetoximino silane.
In some of these embodiments, the coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma- (2, 3-epoxypropyl) propyltrimethoxysilane, and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane.
In some of these embodiments, the catalyst is at least one of di-n-butyl tin dilaurate, di-n-butyl tin diacetate, stannous octoate, di-n-butyl tin dioctoate, propyl titanate, butyl titanate, and titanium chelates.
The invention also provides a preparation method of the silicone sealant.
The specific technical scheme is as follows:
the preparation method of the silicone sealant comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, heavy calcium carbonate, a plasticizer and fumed silica at room temperature to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
In some of the embodiments, the mixing time in step a is 0.5-2 hours, and the stirring time in step b is 1-2 hours.
The invention takes alpha, omega-dihydroxy polydimethylsiloxane, heavy calcium carbonate, fumed silica subjected to dimethyl dichlorosilane hydrophobic treatment and a plasticizer as raw materials, and the raw materials are introduced with a cross-linking agent and a chain extender and are cross-linked under the action of a coupling agent and a catalyst, so that the deketoxime type silicone sealant with high elongation and low modulus and good adhesion to a concrete pavement can be prepared, the prepared silicone sealant still keeps good performance after long-term use under natural conditions, tests show that the surface drying time is 15-25 min, the Shore hardness (Shore A) is 10-18, the tensile strength is 0.8-1.0 MPa, the elongation at break is 900-1100%, the elastic recovery rate is 80-90%, the technical parameter requirements of concrete road joints are completely met, the problem that the existing silicone sealant cannot effectively seal concrete joints for a long time is solved, the quality and the service life of the pavement are improved, thereby effectively maintaining the road traffic safety.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
In the following examples, the viscosity of the α, ω -dihydroxy polydimethylsiloxane at 25 ℃ was 80000 mpa.s; the average grain diameter of the heavy calcium carbonate is 4 mu m, and the water content is lower than 0.1 percent; the fumed silica is subjected to hydrophobic treatment by dimethyldichlorosilane, and the specific surface area of the fumed silica is 175cm2(ii)/g; the plasticizer was dimethicone and had a viscosity of 350mpa.s at 25 ℃.
Example 1
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
α, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 130 portions of
Gas phase process silica: 11 portions of
Dimethyl silicone oil: 50 portions of
Dimethyl dibutylketoximosilane: 2 portions of
Methyl tributyrinoxime silane: 9 portions of
Vinyl tributyrinoxime silane: 3 portions of
Gamma-aminopropyltriethoxysilane: 2 portions of
Di-n-butyl tin dilaurate: 0.1 part
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Example 2
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
α, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 130 portions of
Gas phase process silica: 11 portions of
Dimethyl silicone oil: 50 portions of
Dimethyl dibutylketoximosilane: 4 portions of
Methyl tributyrinoxime silane: 9 portions of
Phenyl tributyrinoxime silane: 3 portions of
Gamma-aminopropyltriethoxysilane: 2 portions of
Di-n-butyl tin dilaurate: 0.1 part
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Example 3
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
α, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 130 portions of
Gas phase process silica: 11 portions of
Dimethyl silicone oil: 50 portions of
Dimethyl dibutylketoximosilane: 6 portions of
Vinyl tributyrinoxime silane: 9 portions of
Phenyl tributyrinoxime silane: 3 portions of
Gamma-glycidoxypropyltriethoxysilane: 2 portions of
Di-n-butyl tin dilaurate: 0.1 part
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Example 4
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
α, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 130 portions of
Gas phase process silica: 11 portions of
Dimethyl silicone oil: 30 portions of
Dimethyl dibutylketoximosilane: 4 portions of
Methyl tributyrinoxime silane: 12 portions of
Gamma-glycidoxypropyltriethoxysilane: 2 portions of
Di-n-butyl tin dilaurate: 0.1 part
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Example 5
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
α, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 130 portions of
Gas phase process silica: 11 portions of
Dimethyl silicone oil: 40 portions of
Dimethyl dibutylketoximosilane: 4 portions of
Vinyl tributyrinoxime silane: 12 portions of
γ - (2, 3-epoxypropyl) propyltrimethoxysilane: 2 portions of
Di-n-butyl tin dilaurate: 0.1 part
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Example 6
A silicone sealant for concrete road joints is prepared from the following raw materials in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
130 portions of heavy calcium carbonate
11 parts of fumed silica
60 parts of dimethyl silicone oil
Dimethyl dibutyl ketoxime silane 4 parts
12 parts of phenyl tributyroximosilane
2 parts of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane
0.1 part of di-n-butyl tin dilaurate
The preparation method of the silicone sealant for the concrete road joint in the embodiment comprises the following steps:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, the ground calcium carbonate, the plasticizer and the fumed silica at room temperature for 1.5 hours to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring for 1.5 hours at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
Comparative example 1
The comparative example provides a silicone sealant for concrete road joints, which is different from the raw material composition in example 1 in that: fumed silica is not hydrophobically treated with dimethyldichlorosilane. The silicone sealant of this comparative example was prepared in the same manner as in example 1.
Comparative example 2
The comparative example provides a silicone sealant for concrete road joints, which is different from the raw material composition in example 1 in that: replacing ground calcium carbonate with nano calcium carbonate (particle size of 20 nm). The silicone sealant of this comparative example was prepared in the same manner as in example 1.
Comparative example 3
The comparative example provides a silicone sealant for concrete road joints, which is different from the raw material composition in example 1 in that: the ground calcium carbonate was replaced by light calcium carbonate (particle size 3 μm). The silicone sealant of this comparative example was prepared in the same manner as in example 1.
Example 7 Performance testing
The performance indexes of the silicone sealants prepared in examples 1 to 6 and comparative examples 1 to 3 were tested: testing the surface dry time according to GB/13477.5; testing the Shore hardness according to GB/T531; testing the tensile strength and the elongation at break according to GB/T528; the elastic recovery rate is tested according to GB/13477.17; the tack adhesion was tested according to GB/13477.10.
The test results are shown in table 1: the elongation at break and the elastic recovery rate of the silicone sealants prepared in examples 1 to 6 are far higher than those of comparative examples, which shows that the elongation at break and the elastic recovery rate of the silicone sealants can be improved by the compound use of the ground limestone and the fumed silica subjected to the hydrophobic treatment by the dimethyldichlorosilane. The combination of the properties of example 6 is the best, the elongation at break and the elastic recovery are the highest, the fixed stretch bonding is not damaged, and the tensile strength, the surface drying time and the hardness are moderate.
TABLE 1 Performance index of Silicone sealants
Figure BDA0001922447750000101
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. The silicone sealant is characterized by being prepared from the following raw materials in parts by weight:
a, ω -dihydroxy polydimethylsiloxane: 100 portions of
Heavy calcium carbonate: 120 to 140 portions of
Gas phase process silica: 9 to 13 portions of
Plasticizer: 30 to 60 portions of
Chain extender: 2 to 6 portions of
A crosslinking agent: 10 to 14 parts by weight of
Coupling agent: 1 to 3 portions of
Catalyst: 0.05-0.15 part;
the gas-phase method silicon dioxide is subjected to hydrophobic treatment by dimethyldichlorosilane;
the average grain diameter of the heavy calcium carbonate is 3.5-5 mu m.
2. The silicone sealant according to claim 1, wherein the viscosity of the a, ω -dihydroxy polydimethylsiloxane at 25 ℃ is 20000 to 100000 mpa.s.
3. The silicone sealant according to claim 1 wherein the ground calcium carbonate has an average particle size of 4 μm and a water content of less than 0.1%.
4. The silicone sealant according to claim 1, wherein the fumed silica has a specific surface area of 150-200 cm2/g。
5. The silicone sealant according to claim 1, wherein the plasticizer is dimethicone having a viscosity of 100 to 1000mPa.s at 25 ℃.
6. The silicone sealant according to any one of claims 1 to 5 wherein the cross-linking agent is at least one of methyl tributyrinoxime silane, vinyl tributyrinoxime silane, phenyl tributyrinoxime silane and tetrabutoximino silane.
7. The silicone sealant according to any one of claims 1 to 5, wherein the chain extender is at least one of dimethyldibutyloximinosilane, methylvinyldibutyloximosilane, methylvinylbis (methylisobutylketonoximino) silane, and methylvinyldiacetoximino silane.
8. The silicone sealant according to any of claims 1 to 5, wherein the coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma- (2, 3-epoxypropyl) propyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane; and/or the presence of a catalyst in the reaction mixture,
the catalyst is at least one of di-n-butyl tin dilaurate, di-n-butyl tin diacetate, stannous octoate, di-n-butyl tin dioctoate, propyl titanate, butyl titanate and titanium chelate.
9. The method for preparing the silicone sealant according to any one of claims 1 to 8, characterized by comprising the steps of:
a. mixing the alpha, omega-dihydroxy polydimethylsiloxane, heavy calcium carbonate, a plasticizer and fumed silica at room temperature to obtain a base material;
b. and adding a chain extender, a cross-linking agent, a coupling agent and a catalyst into the base material, and stirring at room temperature and under the vacuum degree of 0.08-0.1 Mpa to obtain the silicone sealant.
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CN110511596A (en) * 2019-09-09 2019-11-29 青州宇信钙业股份有限公司 A kind of silicone sealant high elongation rate composite Nano filler and preparation method thereof
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CN111793462A (en) * 2020-07-20 2020-10-20 广州市白云化工实业有限公司 Silicone sealant for rail transit and preparation method thereof
CN112662369B (en) * 2020-12-14 2022-11-08 杭州之江新材料有限公司 Transparent silicone sealant and application
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CN104449549A (en) * 2014-12-04 2015-03-25 广州汇纳新材料科技有限公司 Silicone sealant for asphalt road joints and preparation method thereof
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